Milled submicron organic biocides with narrow particle size distribution, and uses thereof

a biocide and submicron technology, applied in the field of producing submicron-sized organic biocides, can solve the problems of posing a health hazard, limiting the use efficiency of organic pesticides, and limiting the application of organic pesticides

Active Publication Date: 2006-04-27
KOPPERS PERFORMANCE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0043] In some instances the second biocide is present in or as an organic liquid. In such cases, the organic liquid can be solubilized in solvent, emulsified in water, and then added to the first biocide before or during milling, or less preferably after milling. The surface of the first biocide can be made compatible with the organic phase of the emulsion, and the liquid or solvated biocide can coat the primary particles. Advantageously, solvent can be withdrawn, for example by venting the gases above the biocidal composition or by drawing a vacuum. The liquid biocide will subsequently be boun

Problems solved by technology

The efficient use of organic pesticides is often restricted by their inherent poor water-solubility.
All of these approaches have drawbacks.
Application of a dust is associated with drift, poses a health hazard, and is inefficient.
Solutions and emulsions that require an organic solvent are undesirable, since the solvent serves no other purpose but to act as a carrier for the product.
As such, the solvent adds an unnecessary cost to the formulation and is an added health risk.
Finally, emulsions are generally unstable and must be prepared at point of use, typically in the hours or minutes before use, and minor changes in the formulation, for example by addition of another biocide, may cause the emulsion to break and separate.
Additionally, particle size reduction below certain values (which depend on the product characteristics) can in the past only be achieved through ex

Method used

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  • Milled submicron organic biocides with narrow particle size distribution, and uses thereof
  • Milled submicron organic biocides with narrow particle size distribution, and uses thereof
  • Milled submicron organic biocides with narrow particle size distribution, and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

Milling Chlorothalonil with 0.5 mm Zirconium Silicate

[0136] The laboratory-sized vertical mill was provided by CB Mills, model# L-3-J. The mill has a 2 liter capacity and is jacketed for cooling. Unless otherwise specified, ambient water was cycled through the mill cooling jacket during operation. The internal dimensions are 3.9″ diameter by 9.1″ height. The mill uses a standard 3×3″ disk agitator (mild steel) on a stainless steel shaft, and it operates at 2,620 rpm.

[0137] The media used in this Example was 0.4-0.5 mm zirconium silicate beads supplied by CB Mills. All particle size determinations were made with a Sedigraph™ 5100T manufactured by Micromeritics, which uses x-ray detection and bases calculations of size on Stokes' Law.

[0138] The formulation contained 20.41% chlorothalonil (98% active), 5% Galoryl™ DT-120, 2% Morwet™ EFW, and 72.6% water by weight, and the concentrate had a pH of 8.0. The total batch weight was about 600 g. The results of a 7.5 hour grinding study ar...

example 2

Milling Chlorothalonil with 0.5 mm Ziconium Oxide

[0141] The same mill and conditions were used in this experiment as in experiment 1. However, the grinding media was 0.5-0.6 mm cerium-doped zirconium oxide beads obtained from CB Mills. The density of the cerium doped zirconium oxide is ˜6.0 g / cm3. The formulation contained 20.41% chlorothalonil (98% Active), 5% Galoryl™ DT-120, 2% Morwet™ EFW, 3% Pluronic™ F-108, and 69.6% water by weight, and the concentrate had a pH of about 7.3. The total batch weight was about 600 g. The results are shown in Table 2 below.

TABLE 2MillingParticle Size Data - Volume %Timed50With Diameter Greater ThanMins.μm10 μm5 μm2 μm1 μm0.4 μm0.2 μm03.448307792——900.31333322—2400.210123 351

[0142] For the higher density 0.5 mm zirconia milling media, a composition with a d50 less than 1 micron and a d95 less than 1 micron was obtainable in 90 minutes, and a composition with a d50 less than 0.3 microns and a d95 less than 0.4 microns was obtainable in 6 hours. ...

example 3

Milling Sparingly Soluble Copper Salts with 0.5 mm Zirconium Silicate

[0143] This comparative example and subsequent example show the effectiveness of the milling media and process on the particle size distribution of inorganic copper salts.

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PUM

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Abstract

A method of milling substantially insoluble solid organic biocides to form a micron or sub-micron product having a narrow particle size distribution is presented. The milling involves wet milling of the organic biocide with high density milling media having a diameter between 0.1 mm and 0.8 mm, preferably between 0.2 mm and 0.7 mm, and a density equal to or greater than 3.8 g/cc, preferably greater than 5.5 g/cc, in a ball mill using between about 40% and 80% loading of the mill volume with milling media, and having the organic biocide suspended in an aqueous milling liquid which comprises one or more surface active agents. The milling speed is preferably high, for example from about 1000 rpm to about 4000 rpm. The milled product can be used in foliar applications at a lower effective dosage than prior art formulations, can be used in improved antifouling paint formulations, and can be used in new applications such as the direct injection of solid organic biocide particulates in wood to act as a long lasting wood preservative.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS [0001] This application claims priority to co-pending U.S. patent application Ser. No. 10 / 868,967 filed Jun. 17, 2004, and to U.S. Provisional Application titled: MILLED SUBMICRON CHLOROTHALONIL WITH NARROW PARTICLE SIZE DISTRIBUTION, AND USES THEREOF, filed on Oct. 8, 2004.STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT [0002] Not applicable INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC [0003] Not applicable SEQUENCE LISTING [0004] Not applicable FIELD OF THE INVENTION [0005] The present invention relates to a method of producing submicron-sized organic biocide particles, methods of packaging same, and uses thereof. More particularly, the invention relates to use of high density milling media having a diameter between 0.1 and 0.8 mm to provide unexpected particle size reduction and narrow particle size distribution even for organic biocides known to be difficult to mill. This milled organic biocidal produc...

Claims

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Application Information

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IPC IPC(8): B02C25/00
CPCA01N25/12B27K3/005B27K3/22B27K3/34B27K3/52A01N59/20A01N37/34
Inventor RICHARDSON, H. WAYNEHODGE, ROBERT L.
Owner KOPPERS PERFORMANCE CHEM
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